CN107674203A - A kind of post-processing approach of polyimide molding powder - Google Patents
A kind of post-processing approach of polyimide molding powder Download PDFInfo
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- CN107674203A CN107674203A CN201711020693.0A CN201711020693A CN107674203A CN 107674203 A CN107674203 A CN 107674203A CN 201711020693 A CN201711020693 A CN 201711020693A CN 107674203 A CN107674203 A CN 107674203A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1003—Preparatory processes
- C08G73/1007—Preparatory processes from tetracarboxylic acids or derivatives and diamines
- C08G73/1028—Preparatory processes from tetracarboxylic acids or derivatives and diamines characterised by the process itself, e.g. steps, continuous
- C08G73/1032—Preparatory processes from tetracarboxylic acids or derivatives and diamines characterised by the process itself, e.g. steps, continuous characterised by the solvent(s) used
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1003—Preparatory processes
- C08G73/1007—Preparatory processes from tetracarboxylic acids or derivatives and diamines
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1042—Copolyimides derived from at least two different tetracarboxylic compounds or two different diamino compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1067—Wholly aromatic polyimides, i.e. having both tetracarboxylic and diamino moieties aromatically bound
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/12—Unsaturated polyimide precursors
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/12—Unsaturated polyimide precursors
- C08G73/124—Unsaturated polyimide precursors the unsaturated precursors containing oxygen in the form of ether bonds in the main chain
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Abstract
The invention discloses a kind of post-processing approach of polyimide molding powder, comprise the following steps：The reaction system of polyimide molding powder after the completion of reaction is filtered, using the organic solvent washing in polyimide molding powder reaction system during filtering, polyimide molding powder is produced after drying.During using the organic solvent used in polyimides preparation system as cleaning solution, it is thus only necessary to which washes can be reclaimed the synthesis for being reused for polyimides by simply removing the entrainer in washes.The treatment process of washes is enormously simplify, reduces polyimide molding powder postprocessing working procedures cost, while the heat endurance of polyimide molding powder can also be improved.
Description
Technical field
The invention belongs to macromolecule material preparation area, and in particular to a kind of post-processing approach of polyimide molding powder.
Background technology
Polyimides, PI is abbreviated as, is the polymer that main chain contains imide group (- C-N-C -).Navigated in universe
Its industry and the application in nuclear power technique and other high temperature resistant fields are more and more wider, e.g., may be used as aircraft spray painting engine part,
Deceleration transmission gear, machine components axle sleeve and seal washer prepare material.Polyimide quantity is with every at this stage
The speed increase in year 8%.
At present, in the production process of polyimide molding powder, usually using methanol or acetone and other organic solvent to system
Standby obtained polyimide molding powder is washed, or replaces washing with substantial amounts of water using above organic solvent, is produced a large amount of
Waste water, cause post processing cost higher, seriously govern the development of polyimides.Such as a kind of 104710789 polyamides of patent CN
In the preparation method of imines Moulding powder, when handling polyimide molding powder, washed using substantial amounts of methanol, ethanol or acetone
Wash；In a kind of polyimides of the A of CN 104231269 and preparation method thereof and polyimide molding powder and using substantial amounts of ethanol
The polyimide molding powder being prepared is washed, produces substantial amounts of waste water.Contain substantial amounts of ethanol or first in the waste water
The complete raw material of unreacted (such as diamines, dianhydride, entrainer, end-capping reagent) and course of reaction in alcohol or acetone, reaction system
In caused accessory substance etc., cause the composition of waste water complex.If to detergent such as the ethanol in waste water, methanol or acetone
When being reclaimed, due to the complicated component of waste water, it is difficult to isolated pure ethanol, methanol or propyl alcohol, and then be difficult to again
Recycled as detergent.And the complicated component of waste water, it is difficult to separate, recycle one by one to each composition, so right
Substantial amounts of human and material resources, financial resources can be not only expended when these waste water are handled, but also the energy can be inevitably present
Waste.So there is the problem of wastewater treatment is difficult, the energy be present waste and processing cost are high in traditional washing methods.
In addition, the heat endurance of traditional polyimide molding powder is not good enough, e.g., 5% thermal weight loss temperature typically 550 DEG C with
Under, it is difficult to reach 560 DEG C or more, constrain application of the polyimides in some hot environments.
In summary, heat endurance existing for polyimide molding powder is not good enough in the prior art, prepares last handling process production
The problem of raw a large amount of waste water improve post processing cost, still lacks effective solution.
The content of the invention
In order to solve the above technical problems, it is an object of the invention to provide a kind of post processing side of polyimide molding powder
Method,
In order to solve the above technical problems, the technical scheme is that：
A kind of post-processing approach of polyimide molding powder, comprises the following steps：
The reaction system of polyimide molding powder after the completion of reaction is filtered, uses polyimide molding during filtering
Organic solvent washing in powder reaction system, polyimide molding powder is produced after drying.
Using the organic solvent used in polyimides preparation system as cleaning solution, containing a large amount of in the filtrate after washing
Organic solvent and a small amount of reaction system in the complete raw material of unreacted (such as diamines, dianhydride, entrainer, end-capping reagent), anti-
Caused accessory substance etc. during answering.Because the amount of by-products in waste water is few, and it is to react when handling waste water
In journey inevitably, the purity of final polyimides will not be affected greatly, so without removing；Reaction system is not
React the diamines in complete raw material, dianhydride is to react the raw material added at the very start, without removing；End-capping reagent in waste water
Amount is seldom, the process of reaction is not interfered with substantially, without removing；Added after the completion of entrainer end-blocking, due in waste water
The amount of entrainer is seldom, if do not remove also will not cause large effect to reaction.If it is considered that when removing, remove in waste water
The relatively simple and easy realization of single material, and the removal degree to the entrainer in waste water requires not tight.
In addition, found by practice, using the organic solvent used in polyimides preparation system as polyimides mould
During the cleaning solution of molding powder, the heat endurance of polyimide molding powder can also be improved, its heat decomposition temperature is reached 560-
580℃。
So if using the organic solvent used in polyimides preparation system as cleaning solution when, it is thus only necessary to will
Entrainer in washes, which simply removes, can reclaim washes the synthesis for being reused for polyimides.It enormously simplify
The treatment process of washes, polyimide molding powder postprocessing working procedures cost is reduced, while polyimides can also be improved
The heat endurance of Moulding powder.
Preferably, the organic solvent in polyimide molding powder reaction system be DMA, N, N- diformazans
One or both of base formamide, dimethyl sulfoxide (DMSO), 1-METHYLPYRROLIDONE, metacresol or isoquinolin or a variety of mixing
Thing.
It is further preferred that the organic solvent is DMA.DMAC N,N' dimethyl acetamide is poly- to improving
Imido thermal stability result is optimal.
A kind of preparation method of polyimides, including above-mentioned post-processing approach.
Preferably, the preparation method of the polyimides, specifically comprises the following steps：
1) under protective atmosphere, aromatic diamine monomer and organic tetracarboxylic dianhydride monomer is mixed in organic solvent, entered
Row prepolymerization reaction；
2) end-capping reagent is added in the solution after prepolymerization reaction, stirring, continues to react；
3) entrainer is added in the reacted solution of step 2), continuously stirs reaction；
4) solution obtained in step 3) is heated up, continues to react, solution occur muddy；
5) by the reacted solution cooling of step 4), filtering, with the organic solvent washing in step 1), produced after drying.
By controlling reaction condition in the preparation method, can complete to test under conditions of catalyst is added without so that
Post-processing approach is easier, and the purity for the polyimide molding powder being prepared is higher.
Reaction monomers, end-capping reagent and entrainer are added separately in the present invention, and often adds one group of raw material and all reacts one section
Time, the reaction of monomer can be made more abundant, the performance of obtained polyimide molding powder is more preferable.
Preferably, in step 1), organic tetracarboxylic dianhydride monomer is pyromellitic acid anhydride (PMDA), bibenzene tetracarboxylic
Dianhydride (BPDA), two methyl phenyl ethers anisole tetracarboxylic dianhydrides (ODPA) or benzophenone tetracarboxylic dianhydride (BTDA).
It is further preferred that organic tetracarboxylic dianhydride monomer is pyromellitic acid anhydride.
Preferably, the aromatic diamine monomer is p-phenylenediamine, m-phenylene diamine (MPD), 4,4 ˊ-diaminodiphenyl ether or diamino
Base diphenyl-methane.
It is further preferred that the aromatic diamine monomer is 4,4 ˊ-diaminodiphenyl ether.
Preferably, in step 1), the organic solvent is DMA, DMF, diformazan
One or both of base sulfoxide, 1-METHYLPYRROLIDONE, metacresol or isoquinolin and a variety of mixtures.
It is further preferred that the organic solvent is DMA.
Preferably, in step 1), the protective atmosphere is inert gas atmosphere.Inert gas is nitrogen, helium, neon
Or argon gas, preferably nitrogen.
Preferably, in step 1), the reaction temperature of prepolymerization reaction is 25-50 DEG C, and the reaction time is 1-3 hours.
Preferably, in step 2), the end-capping reagent is maleic anhydride, ENB acid anhydrides or adjacent PMDA.No
With having different functional groups, after introducing different functional groups, can also continue to and different monomers in the strand of end-capping reagent
Generation hair is answered, or improves the compatibility with other materials.When the present invention uses three kinds of end-capping reagents, to polyimide molding powder
Heat endurance have positive role.
Preferably, in step 2), the temperature of reaction is 25-50 DEG C, and the reaction time is 1-3 hours.
Preferably, in step 3), the entrainer is toluene, dimethylbenzene or triethylamine.
Preferably, in step 3), the temperature of reaction is 25-50 DEG C, and the time of reaction is 1-3 hours.
Preferably, in step 4), the temperature of reaction is 100-180 DEG C, and the time of reaction is 1-8 hours.
Preferably, in step 5), the drying is vacuum drying, and dry temperature is 30-280 DEG C, and the dry time is
11~13h.
The polyimide molding powder that above-mentioned preparation method is prepared.
Beneficial effects of the present invention are：
During using the organic solvent used in polyimides preparation system as cleaning solution, it is thus only necessary to by washes
Entrainer simply remove washes can be reclaimed and be reused for the synthesis of polyimides.It enormously simplify washes
Treatment process, polyimide molding powder postprocessing working procedures cost is reduced, while the heat of polyimide molding powder can also be improved
Stability.
Brief description of the drawings
The Figure of description for forming the part of the application is used for providing further understanding of the present application, and the application's shows
Meaning property embodiment and its illustrate be used for explain the application, do not form the improper restriction to the application.
Fig. 1 is the thermogravimetric curve figure of Moulding powder made from embodiment 1；
Fig. 2 is the glass transition temperature curve map of Moulding powder made from embodiment 1.
Embodiment
It is noted that described further below is all exemplary, it is intended to provides further instruction to the application.It is unless another
Indicate, all technologies used herein and scientific terminology are with usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
It is also intended to include plural form, additionally, it should be understood that, when in this manual using term "comprising" and/or " bag
Include " when, it indicates existing characteristics, step, operation, device, component and/or combinations thereof.
Embodiment 1
20g p-phenylenediamine is dissolved in the solvent of 200ml DMFs, is constantly passed through nitrogen, stirring 2 is small
When.
25g pyromellitic acid anhydride monomers are added portionwise in above-mentioned solution, the interval time added every time is 1 small
When, reacted at room temperature after addition 3 hours.
5g neighbour's PMDA is added in above-mentioned solution, stirred 2 hours at room temperature.
5g toluene is added in above-mentioned solution, after stirring 2 hours, rise temperature is reacted 3 hours to 180 DEG C.
By above-mentioned solution natural cooling, filter, washed repeatedly with DMF.Solvent and filtrate after washing
Distilled, recycle solvent and toluene.
Above-mentioned material is dried 6 hours at 80 DEG C, is dried in vacuo 3 hours.Finally give product.Can be with from Fig. 1
Find out, the thermal weight loss temperature of Moulding powder 5% made from this method illustrates to use Moulding powder made from the inventive method at 565 DEG C
Heat endurance is higher.Fig. 2 gives the glass transition temperature of Moulding powder, can be up to 397 DEG C.
Embodiment 2
30g m-phenylene diamine (MPD)s are dissolved in the solvent of 400ml DMFs, are constantly passed through nitrogen, stirring 2 is small
When.
35g bibenzene tetracarboxylic dianhydride monomers are added portionwise in above-mentioned solution, the interval time added every time is 1 small
When, reacted at room temperature after addition 3 hours.
8g ENB acid anhydrides is added in above-mentioned solution, stirred 2 hours at room temperature.
3g dimethylbenzene is added in above-mentioned solution, after stirring 2 hours, rise temperature is reacted 3 hours to 180 DEG C.
By above-mentioned solution natural cooling, filter, washed repeatedly with DMF.Solvent and filtrate after washing
Distilled, recycle solvent and dimethylbenzene.
Above-mentioned material is dried 6 hours at 80 DEG C, is dried in vacuo 3 hours.Finally give product, polyimide molding
The thermal weight loss temperature of powder 5% is 570 DEG C.
Embodiment 3
By 50g 4,4 ˊ-diaminodiphenyl ether is dissolved in the solvent of 800ml DMAs, is constantly passed through nitrogen
Gas, stir 2 hours.
The methyl phenyl ethers anisole tetracarboxylic dianhydrides of 60g bis- are added portionwise in above-mentioned solution, the interval time added every time is 1 hour,
Reacted at room temperature after addition 3 hours.
7g maleic anhydrides are added in above-mentioned solution, stirred 2 hours at room temperature.
8g triethylamines are added in above-mentioned solution, after stirring 2 hours, rise temperature is reacted 3 hours to 160 DEG C.
By above-mentioned solution natural cooling, filter, washed repeatedly with DMA.Solvent and filtrate after washing
Distilled, recycle solvent and triethylamine.
Above-mentioned material is dried 6 hours at 80 DEG C, is dried in vacuo 3 hours, finally gives product, polyimide molding
The thermal weight loss temperature of powder 5% is 575 DEG C.
Embodiment 4
100g MDAs are dissolved in the solvent of 1000ml DMAs, are constantly passed through nitrogen,
Stirring 2 hours.
80g benzophenone tetracarboxylic dianhydrides are added portionwise in above-mentioned solution, the interval time added every time is 1 hour,
Reacted at room temperature after addition 3 hours.
10g neighbour's PMDA is added in above-mentioned solution, stirred 2 hours at room temperature.
12g triethylamines are added in above-mentioned solution, after stirring 2 hours, rise temperature is reacted 3 hours to 140 DEG C.
By above-mentioned solution natural cooling, filter, washed repeatedly with DMA.Solvent and filtrate after washing
Distilled, recycle solvent and triethylamine.
Above-mentioned material is dried 6 hours at 80 DEG C, is dried in vacuo 3 hours.Finally give product, polyimide molding
The thermal weight loss temperature of powder 5% is 580 DEG C.
Embodiment 5
200g p-phenylenediamine is dissolved in the solvent of 2000ml DMAs, is constantly passed through nitrogen, stirring 2
Hour.
180g bibenzene tetracarboxylic dianhydrides are added portionwise in above-mentioned solution, the interval time added every time is 1 hour, is added
Reacted at room temperature after entering 3 hours.
20g neighbour's PMDA is added in above-mentioned solution, stirred 2 hours at room temperature.
8g triethylamines are added in above-mentioned solution, after stirring 2 hours, rise temperature is reacted 3 hours to 140 DEG C.
By above-mentioned solution natural cooling, filter, washed repeatedly with DMA.Solvent and filtrate after washing
Distilled, recycle solvent and triethylamine.
Above-mentioned material is dried 6 hours at 80 DEG C, is dried in vacuo 3 hours.Finally give product, polyimide molding
The thermal weight loss temperature of powder 5% is 576 DEG C.
Embodiment 6
500g m-phenylene diamine (MPD)s are dissolved in the solvent of 4000ml dimethyl sulfoxide (DMSO)s, are constantly passed through nitrogen, stirred 2 hours.
350g pyromellitic acid anhydrides are added portionwise in above-mentioned solution, the interval time added every time is 1 hour, is added
Reacted at room temperature after entering 3 hours.
80g neighbour's PMDA is added in above-mentioned solution, stirred 2 hours at room temperature.
16g triethylamines are added in above-mentioned solution, after stirring 2 hours, rise temperature is reacted 3 hours to 180 DEG C.
By above-mentioned solution natural cooling, filter, washed repeatedly with dimethyl sulfoxide (DMSO).Solvent after washing is steamed with filtrate
Evaporate, recycle solvent and triethylamine.
Above-mentioned material is dried 6 hours at 80 DEG C, is dried in vacuo 3 hours.Finally give product, polyimide molding
The thermal weight loss temperature of powder 5% is 573 DEG C.
Comparative example 1
A kind of preparation method of polyimide molding powder, the difference with embodiment 1 are：Cleaning solvent is methanol, specifically
Comprise the following steps：
20g p-phenylenediamine is dissolved in the solvent of 200ml DMFs, is constantly passed through nitrogen, stirring 2 is small
When.
25g pyromellitic acid anhydrides are added portionwise in above-mentioned solution, the interval time added every time is 1 hour, is added
Reacted at room temperature after entering 3 hours.
5g neighbour's PMDA is added in above-mentioned solution, stirred 2 hours at room temperature.
5g toluene is added in above-mentioned solution, after stirring 2 hours, rise temperature is reacted 3 hours to 180 DEG C.
By above-mentioned solution natural cooling, filter, washed repeatedly with methanol.Above-mentioned material is dried 6 hours at 80 DEG C,
Vacuum drying 3 hours.Finally give product.5% thermal weight loss temperature of obtained pure Kapton is 545 DEG C.
Comparative example 2
It is with the distinctive points of embodiment 4：The polyimide molding powder being prepared is entered using dimethyl sulfoxide solvent
Row washing, 5% thermal weight loss temperature of dried polyimide molding powder is 576 DEG C.
Comparative example 3
It is with the distinctive points of embodiment 4：The polyimide molding powder being prepared is entered using 1-METHYLPYRROLIDONE
Row washing, 5% thermal weight loss temperature of dried polyimide molding powder is 565 DEG C.
Comparative example 4
It is with the distinctive points of embodiment 4：The polyimide molding powder being prepared is washed using metacresol, done
5% thermal weight loss temperature of the polyimide molding powder after dry is 567 DEG C.
Comparative example 5
It is with the distinctive points of embodiment 4：Using N,N-dimethylformamide to the polyimide molding powder that is prepared
Washed, 5% thermal weight loss temperature of dried polyimide molding powder is 571 DEG C.
The preferred embodiment of the application is the foregoing is only, is not limited to the application, for the skill of this area
For art personnel, the application can have various modifications and variations.It is all within spirit herein and principle, made any repair
Change, equivalent substitution, improvement etc., should be included within the protection domain of the application.
Claims (10)
- A kind of 1. post-processing approach of polyimide molding powder, it is characterised in that：Comprise the following steps：The reaction system of polyimide molding powder after the completion of reaction is filtered, it is anti-using polyimide molding powder during filtering The organic solvent washing in system is answered, is produced after drying.
- 2. post-processing approach according to claim 1, it is characterised in that：It is organic in polyimide molding powder reaction system Solvent is DMAC N,N' dimethyl acetamide, N,N-dimethylformamide, dimethyl sulfoxide (DMSO), 1-METHYLPYRROLIDONE, metacresol or different One or both of quinoline or a variety of mixtures；Preferably, the organic solvent is DMA.
- A kind of 3. preparation method of polyimides, it is characterised in that：Including the post-processing approach of claim 1 or 2.
- 4. preparation method according to claim 3, it is characterised in that：Specifically comprise the following steps：1) under protective atmosphere, aromatic diamine monomer and organic tetracarboxylic dianhydride monomer are mixed in organic solvent, carried out pre- Poly- reaction；2) end-capping reagent is added in the solution after prepolymerization reaction, stirring, continues to react；3) entrainer is added in the reacted solution of step 2), continuously stirs reaction；4) solution obtained in step 3) is heated up, continues to react, solution occur muddy；5) by the reacted solution cooling of step 4), filtering, with the organic solvent washing in step 1), produced after drying.
- 5. preparation method according to claim 4, it is characterised in that：In step 1), organic tetracarboxylic dianhydride monomer is Pyromellitic acid anhydride, bibenzene tetracarboxylic dianhydride, two methyl phenyl ethers anisole tetracarboxylic dianhydrides or benzophenone tetracarboxylic dianhydride, preferably equal benzene four Formic acid dianhydride；Preferably, the aromatic diamine monomer is p-phenylenediamine, m-phenylene diamine (MPD), 4,4 ˊ-diaminodiphenyl ether or diaminourea two Phenylmethane, preferably 4,4 ˊ-diaminodiphenyl ether；Preferably, the organic solvent is DMA, DMF, dimethyl sulfoxide (DMSO), N- methyl One or both of pyrrolidones, metacresol or isoquinolin and a variety of mixtures, preferably DMA.
- 6. preparation method according to claim 4, it is characterised in that：In step 1), the reaction temperature of the prepolymerization reaction For 25-50 DEG C, the reaction time is 1-3 hours.
- 7. preparation method according to claim 4, it is characterised in that：In step 2), the end-capping reagent is maleic anhydride, drop Norbomene anhydride or adjacent PMDA；Preferably, in step 2), the temperature of reaction is 25-50 DEG C, and the reaction time is 1-3 hours；Preferably, in step 3), the entrainer is toluene, dimethylbenzene or triethylamine；Preferably, in step 3), the temperature of reaction is 25-50 DEG C, and the time of reaction is 1-3 hours.
- 8. preparation method according to claim 4, it is characterised in that：In step 4), the temperature of reaction is 100-180 DEG C, The time of reaction is 1-8 hours.
- 9. preparation method according to claim 4, it is characterised in that：In step 5), the drying is vacuum drying, is dried Temperature be 30-280 DEG C, the dry time is 11-13h.
- 10. the polyimide molding powder that any preparation methods of claim 4-9 are prepared.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103113585A (en) * | 2013-03-08 | 2013-05-22 | 哈尔滨工业大学 | Preparation method of solid polyimide microspheres |
| CN104231269A (en) * | 2014-10-14 | 2014-12-24 | 中国科学院长春应用化学研究所 | Polyimide and preparation method thereof and polyimide molding powder |
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